CN207632732U - The purification system of NMP aqueous solutions - Google Patents

The purification system of NMP aqueous solutions Download PDF

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Publication number
CN207632732U
CN207632732U CN201721120448.2U CN201721120448U CN207632732U CN 207632732 U CN207632732 U CN 207632732U CN 201721120448 U CN201721120448 U CN 201721120448U CN 207632732 U CN207632732 U CN 207632732U
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methyl
nmp
pyrrolidone
infiltration evaporation
purification system
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寺师亮辅
山田响介
日比聪
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PRGANO CORP
Organo Corp
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
    • C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D207/24—Oxygen or sulfur atoms
    • C07D207/26—2-Pyrrolidones
    • C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
    • C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/58—Multistep processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/14—Type A
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/20—Faujasite type, e.g. type X or Y
    • C01B39/24—Type Y
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/26—Mordenite type
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/30—Erionite or offretite type, e.g. zeolite T

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  • Chemical & Material Sciences (AREA)
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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Degasification And Air Bubble Elimination (AREA)

Abstract

The utility model provides the purification system of 2 pyrrolidone solution of N methyl.The project of the utility model is the generation for the peroxide for inhibiting NMP in the purification system (1) of NMP aqueous solutions.The purification system (1) of NMP aqueous solutions has the infiltration evaporation film device (201) for water being removed and being generated from NMP aqueous solutions NMP concentrates, it is arranged in the upstream of infiltration evaporation film device (201) or downstream and stores the container (101) of NMP aqueous solutions or NMP concentrates, (103), (106), (301), with by container (101), (103), (106), (301) the inert gas feed mechanism (L401) that gas phase portion is filled with inert gas, (L402), (L403), (L404), (L405), (U402), (U403), (U404), (U405).

Description

The purification system of NMP aqueous solutions
Technical field
The utility model is related to the purification systems of NMP aqueous solutions
Background technology
In the past, it is known that a kind of mixed liquor (hereinafter referred to as NMP from n-methyl-2-pyrrolidone (hereinafter referred to as NMP) and water Aqueous solution) in the method that detaches NMP by pervaporation method (PV methods).PV methods and the side that NMP aqueous solutions are depressurized and distilled Method (distillation under vacuum) is compared, more superior in the performance for saving the energy.In PV methods, there is dividing for compatibility with water using having Infiltration evaporation film device from film (infiltrating and vaporizing membrane).By supplying NMP aqueous solutions in the entrance side of infiltrating and vaporizing membrane and to saturating It crosses side to be depressurized, so as to obtain making NMP aqueous solutions from entrance side to the driving force through side movement.At this point, passing through NMP Poor with the penetration speed of water, mainly water is moved to through side, to carry out the separation (Patent Documents 1 to 3) of NMP and water.
Existing technical literature
Patent document
Patent document 1：Japanese Patent Publication 2013-018747 bulletins
Patent document 2：Japanese Patent Publication 2015-071139 bulletins
Patent document 3：Japanese Patent Publication 2016-030232 bulletins
The purification system for having the NMP aqueous solutions of above-mentioned infiltration evaporation film device is generally configured with for from supply to infiltration vapour Change the subsystem in advance particulate and ion component being removed in the NMP aqueous solutions of film device.The purification system of NMP aqueous solutions has When in the back segment of infiltration evaporation film device be also equipped with ion component, particulate and color for will be eluted from infiltration evaporation film device Spend the subsystem that ingredient removes.In these subsystems, the NMP aqueous solutions before handling and the NMP concentrates after concentration are used The various containers temporarily stored.Have a NMP aqueous solutions or NMP concentrates in the lower storage of container, the top of container by In the variation for the storage capacity for absorbing NMP aqueous solutions or NMP concentrates, therefore become the gas phase portion to be made of air.
Present inventor becomes on above-mentioned such top in the container in gas phase portion, it was found that due to NMP aqueous solutions Or NMP concentration liquid oxidations and generate the peroxide of NMP.If the peroxide of NMP generates, the purity of NMP declines.In addition, If the peroxide of NMP gathers, it is possible to cause to explode.
Utility model content
The purpose of this utility model is to provide a kind of purification system of NMP aqueous solutions, inside store NMP aqueous solutions or NMP concentrates, and NMP aqueous solutions or NMP concentrates are formed with the container at the interface in gas phase portion, the mistake of NMP can be inhibited The generation of oxide.
The purification system of the NMP aqueous solutions including NMP and water of the utility model, which has, removes water from NMP aqueous solutions And the infiltration evaporation film device of NMP concentrates is generated, is arranged in the upstream of infiltration evaporation film device or downstream and stores NMP The container of aqueous solution or NMP concentrates and the inert gas feed mechanism for filling the gas phase portion of container inert gas.
In the otherwise purification system according to the present utility model, the gas phase portion of the container is filled out with nitrogen It fills.
In the otherwise purification system according to the present utility model, have：N-methyl-2-pyrrolidone water Solution supply line, the supply line are connect with the entrance of the infiltration evaporation film device；And heater, the heater are arranged described It is heated on N- N-methyl-2-2-pyrrolidone N aqueous solution supply lines and to the n-methyl-2-pyrrolidone aqueous solution.
In the otherwise purification system according to the present utility model, have：N-methyl-2-pyrrolidone is dense Line is discharged in contracting liquid, which connect with the outlet of the infiltration evaporation film device；And heat exchanger, heat exchanger setting exist The upstream of the heater of the n-methyl-2-pyrrolidone aqueous solution supply line, in the n-methyl-2-pyrrolidone The n-methyl-2-pyrrolidone aqueous solution flowed in aqueous solution supply line is concentrated in the n-methyl-2-pyrrolidone Heat exchange is carried out between the n-methyl-2-pyrrolidone concentrate flowed in liquid discharge line.
In the otherwise purification system according to the present utility model, the infiltration evaporation film device has series connection Multiple infiltration evaporation film modules of connection.
In the otherwise purification system according to the present utility model, having will ooze described at least most downstream Permeate exhausting line of the permeate of vaporization film module back to the upstream side of the infiltration evaporation film device thoroughly.
In the otherwise purification system according to the present utility model, the infiltration evaporation with most downstream The permeate discharge line of film module and the mechanical booster pump being arranged on permeate discharge line.
In the otherwise purification system according to the present utility model, the infiltration evaporation film module of most upstream With the infiltrating and vaporizing membrane being made of the zeolite of CHA types, T-type, Y types or MOR types, the infiltration evaporation film module of the most upstream The infiltration evaporation film module in addition has the infiltrating and vaporizing membrane being made of type A zeolite.
In the otherwise purification system according to the present utility model, have in the infiltration evaporation film device The upstream film exhaust apparatus that removes dissolved oxygen.
In the otherwise purification system according to the present utility model, have be located at the film exhaust apparatus and Ion interchange unit between the infiltration evaporation film device.
In the otherwise purification system according to the present utility model, has and be located at the ion interchange unit The microfiltration film device at least any place between the infiltration evaporation film device and in the upstream of the film exhaust apparatus.
In the otherwise purification system according to the present utility model, has and be located at infiltrating and vaporizing membrane dress The downstream set, and the n-methyl-2-pyrrolidone concentrate is distilled and generates n-methyl-2-pyrrolidone refined solution Distilling apparatus.
In the otherwise purification system according to the present utility model, have：N- methyl-the 2- of process object The receiving slit of pyrrolidone solution；Film exhaust apparatus, the film exhaust apparatus will be included in from described in receiving slit supplies Dissolved oxygen in n-methyl-2-pyrrolidone aqueous solution removes；Stoste slot, which receives is handled by the film exhaust apparatus The n-methyl-2-pyrrolidone aqueous solution crossed, and the n-methyl-2-pyrrolidone aqueous solution is supplied to the infiltration Vaporize film device；Slot is relayed, which receives the n-methyl-2-pyrrolidone concentrated by the infiltration evaporation film device Concentrate；Evaporator, the evaporator make to give birth to from the n-methyl-2-pyrrolidone concentrate evaporation that the relaying slot supplies At n-methyl-2-pyrrolidone purified gases；And condenser, the N- methyl-which will be generated by the evaporator 2-Pyrrolidone purified gases condense and generate n-methyl-2-pyrrolidone refined solution, and the container is the receiving slit, described At least either in film exhaust apparatus, the stoste slot, the relaying slot, the condenser.
The effect of utility model
According to the utility model, due to being formed by inert gas by the gas phase portion of inert gas feed mechanism, container, because This can inhibit the generation of the peroxide of NMP.
Description of the drawings
Fig. 1 is the schematic structural diagram of the purification system of the NMP aqueous solutions of an embodiment according to the present utility model.
Specific implementation mode
Hereinafter, with reference to attached drawing, purification system to the NMP aqueous solutions of an embodiment according to the present utility model and pure Change method illustrates.Fig. 1 shows the general of the purification system 1 of the NMP aqueous solutions of an embodiment according to the present utility model Slightly structure chart.CW indicates that cooling water, BR indicate that brine, ST indicate high-temperature steam in the figure.
NMP is a kind of organic solvent for having high-dissolvability relative to water.NMP is for example in the manufacture work of lithium-ions battery In sequence, electricity is formed the slurry that the particles such as electrode active material disperse will have been made to be coated on electrode collector and made it dry When pole, it is widely used as the decentralized medium of slurry.When making slurry dry, NMP is recovered, and the NMP being recovered is pure It can be recycled after change.The mixed liquor (NMP aqueous solutions) that NMP is for example mixed using water scrubber and as NMP and water is returned It receives.NMP concentration in the NMP aqueous solutions being recovered is about 70~99 weight %.
The purification system 1 of NMP aqueous solutions has in advance remove particulate or ion component from NMP aqueous solutions first Subsystem 100, from the NMP aqueous solutions that particulate or ion component are removed by infiltration evaporation film device by the big portion of moisture Divide and removes and generate the second subsystem 200 of NMP concentrates and NMP concentrates are distilled to and generated third of NMP refined solutions System 300.Hereinafter, illustrating the composition of each subsystem.
(the first subsystem 100)
First subsystem 100 has the receiving slit 101 for the NMP aqueous solutions for receiving the process object being recovered as described above. NMP aqueous solutions by the first NMP aqueous solution supply line L101 being connect with NMP recovering mechanisms (not shown) such as water scrubbers by It is supplied to receiving slit 101.Receiving slit 101 via the 2nd NMP aqueous solution supply line L102 with will be included in NMP aqueous solutions in it is micro- The first microfiltration film device 102 connection that particle removes.It is water-soluble it to be provided with force feed NMP on 2nd NMP aqueous solution supply lines L102 The pump 107 of liquid.First microfiltration film device 102 is arranged in the upstream of film exhaust apparatus 103 (aftermentioned), but can also be arranged Between the downstream of film exhaust apparatus 103, i.e. film exhaust apparatus 103 and ion interchange unit 104 (aftermentioned), alternatively, can also set Set the two between the upstream of film exhaust apparatus 103 and film exhaust apparatus 103 and ion interchange unit 104.
First microfiltration film device 102 is removed via the 3rd NMP aqueous solution supply line L103 with by the dissolved oxygen of NMP aqueous solutions The film exhaust apparatus 103 gone connects.As described later, NMP aqueous solutions are heated to before being imported into infiltration evaporation film device 201 About 120 DEG C.In the NMP aqueous solutions for being heated to about 120 DEG C, NMP be possible to the dissolved oxygen in NMP aqueous solutions in conjunction with and oxygen Change.By in advance removing the dissolved oxygen in NMP aqueous solutions, the oxidation of NMP can be inhibited.In order to monitor the concentration of dissolved oxygen, The arrival line L103 and egress line L104 of film exhaust apparatus 103 are provided with dissolved oxygen instrument (not shown).It is filled in addition, being vented in film The arrival line L103 for setting 103 is provided with moisture teller and resistivity meter (not shown).
The exhaust membrane of film exhaust apparatus 103 can be by polyolefin, polytetrafluoroethylene (PTFE) (PTFE), tetrafluoroethylene-perfluoro alkyl The formation such as vinyl ether co-polymer (PFA), polyurethane, epoxy resin.Since NMP has the property for making a part of organic material dissolving Matter, therefore exhaust membrane is preferably formed by polyolefin, PTFE or PFA.Exhaust membrane is preferably imporosity.In the row of hollow filiform The dissolved oxygen of the NMP aqueous solutions of the internal flow of air film moves under the action of hollow pump 109 to by the external of the exhaust membrane of negative pressure It is dynamic, it is exhausted as a result, that is, carries out the removing of dissolved oxygen.Furthermore it is possible to by inert gases such as nitrogen to the outside of exhaust membrane (gas penetrate side) purging (sweep) reduces partial pressure of oxygen, can also dual-purpose vacuum method and sweeping method.
What film exhaust apparatus 103 was removed via the 4th NMP aqueous solution supply line L104 and by the ion component of NMP aqueous solutions Ion interchange unit 104 connects.Ion interchange unit 104 by anion exchange resin or cation exchange resin by single, Or anion exchange resin is filled with cation exchange resin by mixed bed or multi-compartment bed.In addition, ion exchange resin Type can be any one in gel-type or MR types.Heater 108 sometimes heats NMP aqueous solutions, so that NMP Aqueous solution is supplied to ion interchange unit 104 at a temperature of being suitble to ion exchange.Ion interchange unit 104 is via the 5th NMP aqueous solution supply line L105 are connect with the second microfiltration film device 105.Second microfiltration film device 105 capture be possible to from The resin that ion interchange unit 104 flows out, prevents resin from downstream flowing out.Second microfiltration film device 105 is via the 6th NMP water Solution supply line L106 is connect with stoste slot 106.Stoste slot 106, which receives, passes through film exhaust apparatus 103 and ion interchange unit 104 The NMP aqueous solutions of processing supply the NMP aqueous solutions of reception to infiltration evaporation film device 201.Hereinafter, original will be stored in sometimes Liquid bath 106, supply to infiltration evaporation film device 201 NMP aqueous solutions are known as NMP stostes.
The arrival line L104 and egress line L105 of ion interchange unit 104 are provided with resistivity meter (not shown).Passing through Ion interchange unit 104 processing NMP aqueous solutions resistivity ratio specified value it is small in the case of, that is, ion component is not complete When full removing, NMP aqueous solutions can be made to be recycled along across the path of ion interchange unit 104.Specifically, it is provided with from Five NMP aqueous solutions supply line L105 bifurcateds and the line of return L107 being connect with receiving slit 101.Usual 5th NMP aqueous solutions supply The valve V101 of line L105 is open, and the valve V102 of line of return L107 is closing, but in the resistivity ratio of NMP aqueous solutions In the case that specified value is small, the valve V101 of the 5th NMP aqueous solution supply lines L105 is closed, and opens the valve of line of return L107 V102.It is formed as a result, across receiving slit 101, the first microfiltration film device 102, film exhaust apparatus 103, ion interchange unit 104 Circulating path.It is flowed along the circulating path by NMP aqueous solutions, the ion component being included in NMP aqueous solutions is complete It removes.
In addition, the situation bigger than specified value in the dissolved oxygen of the above-mentioned NMP aqueous solutions handled by film exhaust apparatus 103 Under, that is, when dissolved oxygen is not completely removed, it can also make NMP aqueous solutions along across above-mentioned ion interchange unit 104 Path and recycle.The dissolved oxygen being included in NMP aqueous solutions as a result, is also completely removed.
(the second subsystem 200)
Particulate and ion component are removed and next the NMP stostes being stored in stoste slot 106 are supplied to second Subsystem 200 generates the NMP concentrates that most moisture is removed.Stoste slot 106 is via the 7th NMP aqueous solution supply lines L201 is connect with infiltration evaporation film device 201.7th NMP aqueous solution supply lines L201 is provided with 224 and valve V201 of pump. Seven NMP aqueous solution supply lines L201 are provided with using the primary heater 205 of external steam and positioned at primary heater 205 The Waste Heat Recovery heat exchanger 206 of upstream (primary side), by the primary heater 205 and Waste Heat Recovery heat exchanger 206, NMP aqueous solutions are heated to about 120 DEG C.NMP aqueous solutions by being fed to infiltration evaporation film device 201 are heated to about 120 DEG C, the dewatering of infiltration evaporation film device 201 can be improved.Waste Heat Recovery heat exchanger 206 is water-soluble in the 7th NMP in flowing The NMP aqueous solutions of liquid supply line L201 and flowing carry out heat exchange between the NMP concentrates of NMP concentrates discharge line L204. Primary heater 205 heats NMP aqueous solutions by the steam by external vapour source supply (not shown).Add first The steam supply line of hot device 205 is provided with the valve V202 for adjusting steam delivery volume.It is arranged in the downstream of primary heater 205 There is temperature buzzer display 223.The aperture of valve V202 is adjusted based on the temperature detected by temperature buzzer display 223, NMP water The temperature of solution is controlled in about 120 DEG C.The 7th NMP aqueous solution supply lines L201 Waste Heat Recovery heat exchanger 206 it is upper Trip is provided with flow alarm display 225.The aperture of valve V201 is adjusted based on the flow detected by flow alarm display 225 Whole, the flow of NMP aqueous solutions is controlled in prescribed limit.
Infiltration evaporation film device 201 has the multiple infiltration evaporation film modules being connected in series with.In the present embodiment, 3 Infiltration evaporation film module, i.e. the first infiltration evaporation film module 202, the second infiltration evaporation film module 203, third infiltrating and vaporizing membrane mould Block 204 is connected in series with from upstream toward downstream, but number is not limited to 3.First infiltration evaporation film module 202 is via first Connecting line L202 is connect with the second infiltration evaporation film module 203.Second infiltration evaporation film module 203 is via the second connecting line L203 It is connect with third infiltration evaporation film module 204.First infiltration evaporation film module 202, the second infiltration evaporation film module 203 and third Infiltration evaporation film module 204 be divided by seperation film (infiltrating and vaporizing membrane) 202c, 203c, 204c upstream side enriched chamber 202a, Transmission room 202b, 203b, 204b of 203a, 204a and downstream side.Since seperation film 202c, 203c, 204c have hydrophily, because This makes water penetrate seperation film 202c, 203c, 204c with the penetration speed bigger than NMP.By to through room 202b, 203b, 204b Side applies negative pressure, to through room in the form of steam (gas phase) together with the big water of penetration speed a small amount of NMP small with penetration speed 202b, 203b, 204b are moved, and most NMP stays in enriched chamber 202a, 203a, 204a.Using the principle, water is water-soluble from NMP It is detached in liquid.In the exit of third infiltration evaporation film module 204, NMP concentration can be obtained and be raised to about 99.99% NMP concentrates (moisture be less than 0.01%).
NMP aqueous solutions flow successively through the first infiltration evaporation film module 202, the second infiltration evaporation film module 203 and third and ooze Film module 204 is vaporized thoroughly, and the moisture in NMP aqueous solutions is gradually removed.As described above, in order to maintain the removal efficiency of moisture, It is respectively arranged with secondary heater 207 and third heater 208 in the first connecting line L202 and the second connecting line L203.Second adds Hot device 207 and third heater 208 are heat exchangers as primary heater 205, by by external vapour source supply NMP aqueous solutions are heated to about 120 DEG C by steam.It is set respectively in the steam supply line of secondary heater 207 and third heater 208 It is equipped with valve V203, V204 for adjusting steam delivery volume.The NMP concentrates being discharged from third infiltration evaporation film module 204 are logical Cross the relaying slot 301 that NMP concentrates discharge line L204 is supplied to third subsystem 300.As described above, being arranged in NMP concentrates The NMP concentrates flowed in outlet L204 are by Waste Heat Recovery heat exchanger 206 and in the 7th NMP aqueous solution supply lines L201 Heat exchange is carried out between the NMP aqueous solutions of middle flowing, NMP aqueous solutions are preheated.
It is provided with the line of return of NMP concentrates that line L204 bifurcateds are discharged from NMP concentrates and are connect with stoste slot 106 L215.In general, the valve V205 of NMP concentrates discharge line L204 is open, the valve V206 of line of return L215 is to close, NMP Concentrate is supplied to relaying slot 301.On the other hand, the case where can not supply NMP concentrates to relaying slot 301 etc. Under, valve V205 is to close, and valve V206 is open, and NMP concentrates return to stoste slot 106.In addition, being concentrated by NMP In the case that liquid sends stoste slot 106 back to, by the way that the cooler 226 in line of return L215 is arranged, cooled down by cooling water, so that The temperature of NMP concentrates becomes degree identical with the temperature of NMP aqueous solutions (stoste).
First infiltration evaporation film module 202, the second infiltration evaporation film module 203, third infiltration evaporation film module 204 it is saturating It crosses room 202b, 203b, 204b and line L206, the second permeate discharge line L209, third transmission is discharged by the first permeate respectively Liquid is discharged line L212 and is connect through liquid case 216 through liquid case 215, third through liquid case 214, second with first.The water of gas phase and A small amount of NMP is condensed by cooling water or brine, is then collected at first and is penetrated liquid case through liquid case 214, second 215, third penetrates the bottom of liquid case 216.Specifically, cooling water or brine penetrate liquid case 214, the second permeate in covering first Through flowing in the coolant jacket (not shown) around liquid case 216, water and NMP to gas phase carry out cold insulation for case 215, third, into And by cooling line L207, L210, L213, setting is supplied in the first permeate discharge line L206, the discharge of the second permeate Line L209, the first heat exchanger 211 of third permeate discharge line L212, second heat exchanger 212, third heat exchanger 213, The water and NMP of gas phase are condensed.The temperature of brine is preferably 0~-20 DEG C.First through liquid case 214, the second permeate Case 215, third are connected separately with the first condensed water discharge line L208, the second condensed water discharge line through the bottom of liquid case 216 Line L214 is discharged in L211, third condensed water, cold in the first condensed water discharge line L208, the second condensed water discharge line L211, third Condensate discharge line L214 is respectively arranged with the first discharge pump 220, the second discharge pump 221, third discharge pump 222.The water being condensed Liquid case 214, second is penetrated from first by the first discharge pump 220, the second discharge pump 221, third discharge pump 222 with a small amount of NMP It is discharged through liquid case 216 through liquid case 215, third.In addition, penetrating liquid case 215, third through liquid case 214, second first It is provided with to the first vacuum pump 217, the second vacuum for applying negative pressure through room 202b, 203b, 204b through the top of liquid case 216 Pump 218, third vacuum pump 219.
The infiltration evaporation film module of most upstream, i.e. the first infiltration evaporation film module 202 have by CHA types, T-type, Y types or The infiltrating and vaporizing membrane 202c that the zeolite of MOR types is constituted.Infiltration evaporation film module other than the infiltration evaporation film module of most upstream, i.e., Second infiltration evaporation film module 203, third infiltration evaporation film module 204 have the infiltrating and vaporizing membrane being made of type A zeolite 203c、204c.Type A zeolite more at a low price and dewatering is high, but the case where handling moisture concentration high NMP aqueous solutions Under, leakage or degraded performance easily occurs.In contrast, the zeolite other than A types can keep longer-term intersexuality in above-mentioned environment Energy.Therefore, the first infiltration evaporation film module 202 handled the NMP aqueous solutions of the water containing 10~20 weight % oozes Vaporization film 202c uses the zeolite of CHA types, T-type, Y types or MOR types thoroughly, what the NMP aqueous solution few to moisture was handled Second infiltration evaporation film module 203, third infiltration evaporation film module 204 infiltrating and vaporizing membrane 203c, 204c use A types boiling Stone.In addition, the multiple infiltrating and vaporizing membranes for constituting the first infiltration evaporation film module 202 need not be all by CHA types, T-type, Y types Or the zeolite of MOR types is constituted, a part of film can also be made of type A zeolite.
Third permeate discharge line L212 is provided with cooler 209 and mechanical booster pump 210.Cooler 209 will be from The permeate of three infiltration evaporation film modules 204 discharge is pre-chilled.Mechanical booster pump 210 and cooler 209 are in order to third Infiltration evaporation film module 204 applies big negative pressure through room 204b and is arranged.It supplies to third infiltration evaporation film module 204 NMP aqueous solutions moisture amount it is considerably less, therefore, not only by third vacuum pump 219 and pass through mechanical booster pump 210 apply enough negative pressure, can effectively detach water from NMP aqueous solutions.Cooler 209 and mechanical booster pump 210 It can be omitted.In addition, between cooler 209 and mechanical booster pump 210, can also be arranged cold by cooler 209 for storing The crucible (not shown) of solidifying condensed water.
Second infiltration evaporation film module 203, third infiltration evaporation film module 204 permeate be recycled to infiltrating and vaporizing membrane The upstream side of device 201.Specifically, the second condensed water discharge line L211, third condensed water discharge line L214 and permeate recycle Line L205 connections, permeate exhausting line L205 are connect with stoste slot 106.From the second condensed water discharge line L211, third condensed water The permeate of line L214 discharges is discharged compared with the permeate being discharged from the first condensed water discharge line L208, the amount of NMP is high, Therefore, by being recycled to it, the rate of recovery of NMP can be improved.Recycling has the infiltration evaporation film module of permeate unlimited Due to the second infiltration evaporation film module 203, third infiltration evaporation film module 204, as long as at least infiltrating and vaporizing membrane mould of most downstream The permeate of block (third infiltration evaporation film module 204) is recycled to the upstream side of infiltration evaporation film device 201.Permeate It can also be recovered to receiving slit 101, it can also be by the way that Y-track (not shown) be arranged in permeate exhausting line L205, selectively It is recovered to stoste slot 106 and receiving slit 101.
(third subsystem 300)
It is removed most moisture in the NMP concentrates that the second subsystem 200 generates.But due to NMP concentrates Including the particulate of micro chromatic component or infiltrating and vaporizing membrane 202c, 203c, 204c for being eluted from infiltration evaporation film module and Ion component, therefore distilled in turn by the third subsystem 300 positioned at the downstream of infiltration evaporation film device 201, to raw At NMP refined solutions.In addition, following third subsystems 300 uses simple distillation mode, but NMP concentrates can carried out Distillating method is not limited in the range of distillation.It is, for example, possible to use precise distillation mode.But, dress few based on energy consumption Set that size is small, reasons, the simple distillation mode such as easy to operate are preferred.In addition, even if in simple distillation mode, in this embodiment party Decompression simple distillation mode used in formula is special recommendation from the viewpoint of it can prevent heat deterioration.
As described above, NMP concentrates are stored in relaying slot 301 for the time being.Third subsystem 300 is independently of the second subsystem Subsystem, for example, there may come a time when to be used as follows, by the fortune of third subsystem 300 in the operating of the second subsystem 200 Turn to temporarily cease.Therefore, slot 301 is relayed by setting, so as to tie up the second subsystem 200 with third subsystem 300 While holding mutual independence, more flexibly use.Relaying slot 301 is via the first NMP concentrate supply line L301 and again Raw device 302 connects.First NMP concentrate supply lines L301 is provided with 306 and valve V301 of pump.Regenerator 302 is heat exchange Device carries out hot friendship between the NMP concentrates (hereinafter referred to as NMP purified gases) evaporated by aftermentioned evaporator 303 It changes.Thereby, it is possible to reduce the thermic load of evaporator 303.Regenerator 302 is via the 2nd NMP concentrate supply line L302 and evaporation Tank 303 connects.Evaporator 303 is by heating NMP concentrates from the steam of external vapour source supply (not shown) Make its evaporation.The steam supply line of evaporator 303 is provided with the valve V302 for adjusting steam delivery volume.In evaporator 303 Bottom be detained have high temperature liquid phase NMP concentrates, be formed with the NMP purified gas for the gas phase for being removed particulate at an upper portion thereof Body.Since the chromatic component of the NMP concentrates included in liquid phase also has the property of difficult evaporation, evaporator 303 is accumulated in Bottom.In addition, the evaporator 303 as present embodiment, illustrates by taking falling film type evaporation tank as an example, but also may be used below To use the evaporator other than falling film type, such as the rapidly evaporators such as formula, shell and tube.Connect in the bottom and top of evaporator 303 It is connected to circular route L303, extract the NMP concentrates of liquid phase and returns to evaporator 303, the cycle quilt heated again using falling liquid film It operates repeatedly.It is provided in the bottom of steam extraction tank 304 (aftermentioned) and extracts line with the NMP concentrates at the interflow circular route L303 L306.The NMP concentrates for being trapped in the bottom of steam extraction tank 304 extract line L306 and circular route also by NMP concentrates L303 and return to evaporator 303, be heated again.Circular route L303 is provided with circulating pump 307 and valve V303.From circular route L303 bifurcateds go out to be provided with the discharge line L309 of the NMP concentrates of valve V304.
The NMP purified gases of evaporator 303 are extracted from the gas phase portion of evaporator 303, pass through the first NMP purified gases It extracts line L304 and is extracted to steam extraction tank 304.Steam extraction tank 304 is via the 2nd NMP purified gases extraction line L305 It is connect with regenerator 302.The heat of NMP purified gases carries out heat exchange in regenerator 302 and the NMP concentrates of liquid phase.From regeneration The NMP purified gases that device 302 is gone out extract line L307 by the 3rd NMP purified gases in turn and are directed to condenser 305, cold But water condensation becomes NMP purified waters.It is connected with NMP purifications in the outlet of condenser 305 and is piped L308.NMP purified waters are logical Cross be arranged NMP purifications be piped L308 pump 308 be discharged to outside the system of purification system 1 of NMP aqueous solutions.
(inert gas feed mechanism)
The purification system 1 of the NMP aqueous solutions of present embodiment is also equipped with the gas phase portion inert gas filling of container Inert gas feed mechanism.As described above, infiltration evaporation film device 201 upstream and downstream be provided with storage NMP aqueous solutions, The various containers of NMP concentrates or NMP refined solutions.Several in these containers form NMP aqueous solutions, NMP concentrations in inside The interface of liquid or NMP refined solutions and gas phase portion.As the container for meeting the condition, enumerated below.
(1) receiving slit 101 of NMP aqueous solutions
(2) stoste slot 106
(3) slot 301 is relayed
(4) regenerator 302
(5) evaporator 303
(6) steam extraction tank 304
(7) condenser 305
The gas phase portion of these previous containers 101,106,301~305 is formed by air.But inventor has found at this Filling in a little containers (in the following record about inert gas feed mechanism, container refers to container 101,106,301~305) In the case of air, NMP is combined with the air in gas phase portion, generates the peroxide (NMP-O-O-H of NMP；5- hydroperoxidations -1- N-methyl-2-2-pyrrolidone N).If the peroxide of NMP gathers, it is likely that explode.Then, in the present embodiment, exist These containers are provided with inert gas feed mechanism.As inert gas, nitrogen is preferred, can also use argon gas.Inertia Gas supply mechanism supplies main pipe L401, from main pipe L401 bifurcateds to each supply for receptacles inertia from inert gas as described below Sealing gland unit in each inert gas supply line is arranged in the inert gas supply line of gas.
Specifically, it is connected with inert gas in the supply source of inert gas (not shown) and supplies main pipe L401, inert gas Supply main pipe L401 and receiving slit 101, stoste slot 106, relaying slot 301 respectively by inert gas supply line L402, L403, L404 connections.Inert gas supply line L402, L403, L404 are connected to the top of container.Inert gas supply line L402, L403, L404 are respectively arranged with sealing gland unit U402, U403, U404.It is provided with the vacuum pump 309 being connect with condenser 305, Piping between condenser 305 and vacuum pump 309 is connected with the inert gas supply line L405 of purging.Inert gas is from inertia Gas feed line L405 is supplied to condenser 305, so inert gas by line L307, L302, L304, L305 to regenerator 302, evaporator 303, steam extraction tank 304 supply.Although diagram omit, can also regenerator 302, evaporator 303, The inert gas supply line of same vacuum pump and purging is arranged in steam extraction tank 304.Next with sealing gland unit U402, It is illustrated for U403, U404, but is also same about other sealing gland units.Sealing gland unit U402, U403, U404 It is automatically opened in the pressure reduction of the container in downstream side, so that inert gas fills container.Therefore, if NMP water in container The amount of solution, NMP concentrates and NMP refined solutions lowers, then the pressure of container declines, by sealing gland unit U402, U403, U404, inert gas are filled into container.
Inert gas is filled into when the purification system 1 of NMP aqueous solutions initial starts up in container.At this point, due to container Inside filled up by air, inert gas is sent by container by sealing gland unit U402, U403, U404, forcibly by container Internal air is replaced as inert gas.
By the way that inert gas is filled into container, the possibility of the explosion of NMP peroxide can not only be reduced, additionally it is possible to Inhibit the amount of moisture and dissolved oxygen amount that are dissolved in NMP aqueous solutions in container, NMP concentrates and NMP refined solutions.Its result, which can mitigate, oozes The load of vaporization film module thoroughly.Further, since there's almost no oxygen in container, thus can also obtain preventing NMP aqueous solutions, The effect of the oxidation of NMP concentrates and NMP refined solutions.
(embodiment)
NMP aqueous solutions are filled into container, then measure the peroxide concentrations in the NMP aqueous solutions that top is gas phase Time-varying.Gas phase is set as nitrogen (99.9 weight % of ＞ or more) by embodiment, and gas phase is set as air by comparative example.To be filled in container The state of NMP aqueous solutions and nitrogen or air is placed 30, and the concentration of NMP peroxide is measured according to iodimetry.It will knot Fruit is shown in table 1.It can confirm as a result, by being nitrogen, the concentration of the NMP peroxide in NMP aqueous solutions by vapor-phase replacement It is suppressed to substantially 0.
[table 1]
Symbol description：
The purification system of 1 NMP aqueous solutions
100 first subsystems
101 receiving slits
102 first microfiltration film devices
103 film exhaust apparatus
104 ion interchange units
105 second microfiltration film devices
106 stoste slots
107 pumps
108 heaters
The NMP aqueous solution supply lines of L101~L106 first~the 6th
The L107 lines of return
V101,102 valves
200 second subsystems
201 infiltration evaporation film devices
202~204 first~third infiltrating and vaporizing membrane film blocks
The enriched chamber 202a, 203a, 204a
202b, 203b, 204b penetrate room
202c, 203c, 204c seperation film (infiltrating and vaporizing membrane)
205 primary heaters
206 Waste Heat Recovery heat exchangers
207 secondary heaters
208 third heaters
209 coolers
210 mechanical booster pumps
211,212,213 first~third heat exchanger
214,215,216 first~thirds penetrate liquid case
217,218,219 first~third vacuum pump
220,221,222 first~third discharge pump
223 temperature buzzer displays
224 pumps
225 flow alarm displays
226 coolers
The 7th NMP aqueous solution supply lines of L201
The first, second connecting line of L202, L203
Line is discharged in L204 NMP concentrates
L205 permeate exhausting lines
Line is discharged in L206, L209, L212 first~third permeate
L207, L210, L213 cooling line
Line is discharged in L208, L211, L214 first~third condensed water
The line of return of L215 NMP concentrates
V201~V206 valves
300 third subsystems
301 relaying slots
302 regenerators
303 evaporators
304 steam extraction tanks
305 condensers
306 pumps
307 circulating pumps
308 pumps
The first NMP concentrate supply lines of L301
The 2nd NMP concentrate supply lines of L320
L303 circular routes
The first NMP purified gases of L304 extract line
The 2nd NMP purified gases of L305 extract line
L306 NMP concentrates extract line
The 3rd NMP purified gases of L307 extract line
The extraction piping of L308 NMP purified waters
The discharge line of L309 NMP concentrates
V301~V304 valves
L401 inert gases supply main pipe
L402, L403, L404 inert gas supply line
U402, U403, U404 sealing gland unit.

Claims (13)

1. a kind of purification system, be include n-methyl-2-pyrrolidone and water n-methyl-2-pyrrolidone aqueous solution it is pure Change system, which is characterized in that it has：
Infiltration evaporation film device, the infiltration evaporation film device from the n-methyl-2-pyrrolidone aqueous solution by water remove and Generate n-methyl-2-pyrrolidone concentrate；
Container, the container are arranged in the upstream or downstream of the infiltration evaporation film device, store the n-methyl-2-pyrrolidone Aqueous solution or the n-methyl-2-pyrrolidone concentrate；
Inert gas feed mechanism, the mechanism fill in the gas phase portion of the container with inert gas.
2. purification system according to claim 1, which is characterized in that the gas phase portion of the container is filled with nitrogen.
3. purification system according to claim 1 or 2, which is characterized in that it has：
N-methyl-2-pyrrolidone aqueous solution supply line, the supply line are connect with the entrance of the infiltration evaporation film device；With
Heater, the heater are arranged on the n-methyl-2-pyrrolidone aqueous solution supply line and to the N- methyl -2- Pyrrolidone solution heats.
4. purification system according to claim 3, which is characterized in that it has：
Line is discharged in n-methyl-2-pyrrolidone concentrate, which connect with the outlet of the infiltration evaporation film device；With
The heater in the n-methyl-2-pyrrolidone aqueous solution supply line is arranged in heat exchanger, the heat exchanger Upstream, the n-methyl-2-pyrrolidone aqueous solution flowed in the n-methyl-2-pyrrolidone aqueous solution supply line with The n-methyl-2-pyrrolidone concentrate be discharged in line between the n-methyl-2-pyrrolidone concentrate that flows into Row heat exchange.
5. purification system according to claim 1, which is characterized in that the infiltration evaporation film device, which has, to be connected in series with Multiple infiltration evaporation film modules.
6. purification system according to claim 5, which is characterized in that it has the infiltration evaporation of at least most downstream Permeate exhausting line of the permeate of film module back to the upstream side of the infiltration evaporation film device.
7. purification system according to claim 5 or 6, which is characterized in that its described infiltrating and vaporizing membrane with most downstream The permeate discharge line of module and the mechanical booster pump being arranged on permeate discharge line.
8. purification system according to claim 5, which is characterized in that the infiltration evaporation film module of most upstream have by The infiltrating and vaporizing membrane that constitutes of zeolite of CHA types, T-type, Y types or MOR types, the institute other than the infiltration evaporation film module of the most upstream Stating infiltration evaporation film module has the infiltrating and vaporizing membrane being made of type A zeolite.
9. purification system according to claim 1, which is characterized in that it has in the upstream of the infiltration evaporation film device The film exhaust apparatus that dissolved oxygen is removed.
10. purification system according to claim 9, which is characterized in that it has positioned at the film exhaust apparatus and described Ion interchange unit between infiltration evaporation film device.
11. purification system according to claim 10, which is characterized in that it, which has, is located at the ion interchange unit and institute State the microfiltration film device at least any place between infiltration evaporation film device and in the upstream of the film exhaust apparatus.
12. purification system according to claim 1, which is characterized in that it has positioned at the infiltration evaporation film device Downstream, and the n-methyl-2-pyrrolidone concentrate is distilled and is generated the steaming of n-methyl-2-pyrrolidone refined solution Distillation unit.
13. purification system according to claim 1, which is characterized in that it has：
The receiving slit of the n-methyl-2-pyrrolidone aqueous solution of process object；
Film exhaust apparatus, the film exhaust apparatus will be included in the n-methyl-2-pyrrolidone water supplied from the receiving slit Dissolved oxygen in solution removes；
Stoste slot, the stoste slot are received by the processed n-methyl-2-pyrrolidone aqueous solution of the film exhaust apparatus, and The n-methyl-2-pyrrolidone aqueous solution is supplied to the infiltration evaporation film device；
Slot is relayed, which receives the n-methyl-2-pyrrolidone concentrate concentrated by the infiltration evaporation film device；
Evaporator, the evaporator make to generate from the n-methyl-2-pyrrolidone concentrate evaporation that the relaying slot supplies N-methyl-2-pyrrolidone purified gases；With
The n-methyl-2-pyrrolidone purified gases generated by the evaporator are condensed and are given birth to by condenser, the condenser At n-methyl-2-pyrrolidone refined solution,
The container is in the receiving slit, the film exhaust apparatus, the stoste slot, the relaying slot, the condenser At least either.
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